#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:35:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179337 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/34/4323434.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4323434
loop_
_publ_author_name
'F. Albert Cotton'
'Günter Schmid'
_publ_section_title
;
 Mononuclear Molybdenum(IV) Complexes with Two Multiply Bonded Chalcogen
 Ligands in Trans Configuration and Chelating Biphosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2267
_journal_page_last               2278
_journal_paper_doi               10.1021/ic961071v
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        'Reac. of MoOCl(dppee)2/Li2S methanol/air'
_chemical_formula_analytical     'FAB (M+H)+ at 923u'
_chemical_formula_moiety         'C52 H44 Mo1 O2 P4, 2 (C H4 O)'
_chemical_formula_structural
;
 Mo (O)2 ( (C6 H5)2 P C H C H P (C6 H5)2 )2, 2 (C H3 O H)
;
_chemical_formula_sum            'C54 H52 Mo O4 P4'
_chemical_formula_weight         984.84
_chemical_name_common            'trans-Mo(O)₂(dppee)₂, 2 CH₃OH'
_chemical_name_systematic
;
trans-bis(cis-1,2-bis(diphenylphosphino)ethylene-P,P')-di-oxo-molybdenum(IV) 
methanol solvate
;
_chemical_temperature_decomposition 433
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.999(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1340(15)
_cell_length_b                   18.435(2)
_cell_length_c                   12.515(2)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      13.0
_cell_volume                     2398.2(6)
_computing_cell_refinement       'LCR out of package ULM'
_computing_data_collection       'Enraf Nonius CAD4 software'
_computing_data_reduction        STP
_computing_molecular_graphics    'ORETP out package ULM'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Mo in position 0.0 0.0 0.0'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       ω/θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0305
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3949
_diffrn_reflns_theta_max         23.94
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9677
_exptl_absorpt_correction_type   \Y-Scans
_exptl_crystal_colour            'light yellow-orange'
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not done'
_exptl_crystal_description       'thick plate with brownish inclusions'
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_obs          0.0323
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0367P)²+2.1818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0872
_refine_ls_wR_factor_obs         0.0796
_reflns_number_observed          3045
_reflns_number_total             3759
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961071v_1.cif
_cod_data_source_block           MoO2dppee2_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (10 times).

'_geom_bond_publ_flag' value 'N'
changed to 'n' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (26
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (14 times).

'_geom_angle_publ_flag'
value 'N' changed to 'n' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29
(38 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not done' was changed to '?' -
the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+2.1818P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+2.1818P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2398.3(5)
_cod_database_code               4323434
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mo1 Mo 0.0000 0.0000 0.0000 0.02514(11) Uani 1 d S .
O1 O 0.1398(2) 0.02972(11) 0.1180(2) 0.0346(5) Uani 1 d . .
P1 P -0.11225(7) 0.00331(4) 0.14168(6) 0.0302(2) Uani 1 d . .
P2 P -0.06665(7) 0.13049(4) -0.01676(6) 0.0303(2) Uani 1 d . .
C1 C -0.1443(3) 0.0983(2) 0.1628(3) 0.0389(7) Uani 1 d . .
C1A C -0.0169(3) -0.0247(2) 0.2868(2) 0.0323(6) Uani 1 d . .
C1B C -0.0327(3) -0.0930(2) 0.3266(3) 0.0429(8) Uani 1 d . .
H1B H -0.0970(3) -0.1236(2) 0.2809(3) 0.069(3) Uiso 1 calc R .
C1C C 0.0464(3) -0.1155(2) 0.4337(3) 0.0531(9) Uani 1 d . .
H1C H 0.0346(3) -0.1610(2) 0.4605(3) 0.069(3) Uiso 1 calc R .
C1D C 0.1422(4) -0.0713(2) 0.5008(3) 0.0553(9) Uani 1 d . .
H1D H 0.1962(4) -0.0871(2) 0.5725(3) 0.069(3) Uiso 1 calc R .
C1E C 0.1590(4) -0.0040(2) 0.4630(3) 0.0554(9) Uani 1 d . .
H1E H 0.2240(4) 0.0260(2) 0.5092(3) 0.069(3) Uiso 1 calc R .
C1F C 0.0792(3) 0.0197(2) 0.3556(3) 0.0441(8) Uani 1 d . .
H1F H 0.0907(3) 0.0657(2) 0.3302(3) 0.069(3) Uiso 1 calc R .
C1G C -0.2676(3) -0.0394(2) 0.1153(3) 0.0377(7) Uani 1 d . .
C1H C -0.3237(3) -0.0776(2) 0.0169(3) 0.0593(10) Uani 1 d . .
H1H H -0.2832(3) -0.0811(2) -0.0363(3) 0.069(3) Uiso 1 calc R .
C1I C -0.4414(4) -0.1112(3) -0.0039(4) 0.088(2) Uani 1 d . .
H1I H -0.4799(4) -0.1368(3) -0.0717(4) 0.069(3) Uiso 1 calc R .
C1K C -0.5008(4) -0.1074(3) 0.0728(5) 0.0809(14) Uani 1 d . .
H1K H -0.5796(4) -0.1303(3) 0.0577(5) 0.069(3) Uiso 1 calc R .
C1L C -0.4458(4) -0.0701(3) 0.1720(4) 0.0786(13) Uani 1 d . .
H1L H -0.4865(4) -0.0676(3) 0.2251(4) 0.069(3) Uiso 1 calc R .
C1M C -0.3289(4) -0.0359(2) 0.1937(3) 0.0641(11) Uani 1 d . .
H1M H -0.2912(4) -0.0104(2) 0.2617(3) 0.069(3) Uiso 1 calc R .
C2 C -0.1263(3) 0.1500(2) 0.0983(3) 0.0395(7) Uani 1 d . .
C2A C 0.0605(3) 0.19789(15) 0.0093(2) 0.0336(6) Uani 1 d . .
C2B C 0.1419(3) 0.2109(2) 0.1203(3) 0.0476(8) Uani 1 d . .
H2B H 0.1292(3) 0.1865(2) 0.1804(3) 0.069(3) Uiso 1 calc R .
C2C C 0.2421(3) 0.2597(2) 0.1430(3) 0.0596(10) Uani 1 d . .
H2C H 0.2962(3) 0.2683(2) 0.2181(3) 0.069(3) Uiso 1 calc R .
C2D C 0.2619(3) 0.2956(2) 0.0549(4) 0.0590(10) Uani 1 d . .
H2D H 0.3288(3) 0.3289(2) 0.0703(4) 0.069(3) Uiso 1 calc R .
C2E C 0.1834(3) 0.2826(2) -0.0558(3) 0.0542(9) Uani 1 d . .
H2E H 0.1979(3) 0.3065(2) -0.1155(3) 0.069(3) Uiso 1 calc R .
C2F C 0.0821(3) 0.2338(2) -0.0793(3) 0.0429(8) Uani 1 d . .
H2F H 0.0288(3) 0.2252(2) -0.1547(3) 0.069(3) Uiso 1 calc R .
C2G C -0.1951(3) 0.1661(2) -0.1424(3) 0.0372(7) Uani 1 d . .
C2H C -0.2381(3) 0.1250(2) -0.2404(3) 0.0488(8) Uani 1 d . .
H2H H -0.2041(3) 0.0790(2) -0.2408(3) 0.069(3) Uiso 1 calc R .
C2I C -0.3318(4) 0.1515(2) -0.3383(3) 0.0633(10) Uani 1 d . .
H2I H -0.3600(4) 0.1235(2) -0.4045(3) 0.069(3) Uiso 1 calc R .
C2K C -0.3829(4) 0.2187(2) -0.3378(4) 0.0692(12) Uani 1 d . .
H2K H -0.4452(4) 0.2367(2) -0.4040(4) 0.069(3) Uiso 1 calc R .
C2L C -0.3426(4) 0.2596(2) -0.2405(4) 0.0744(13) Uani 1 d . .
H2L H -0.3787(4) 0.3050(2) -0.2402(4) 0.069(3) Uiso 1 calc R .
C2M C -0.2487(3) 0.2339(2) -0.1426(3) 0.0599(10) Uani 1 d . .
H2M H -0.2212(3) 0.2622(2) -0.0766(3) 0.069(3) Uiso 1 calc R .
H1 H -0.1786(31) 0.1084(17) 0.2226(28) 0.050(7) Uiso 1 d . .
H2 H -0.1441(31) 0.1960(19) 0.1066(27) 0.050(7) Uiso 1 d . .
O3 O 0.3231(4) 0.0878(3) 0.3044(4) 0.141(2) Uani 1 d . .
C3A C 0.4284(13) 0.0984(7) 0.3044(11) 0.101(3) Uiso 0.50 d P .
H3A1 H 0.4234(13) 0.1281(32) 0.2399(36) 0.125(16) Uiso 0.50 calc PR .
H3A2 H 0.4681(28) 0.0529(7) 0.2995(61) 0.125(16) Uiso 0.50 calc PR .
H3A3 H 0.4788(23) 0.1228(34) 0.3738(29) 0.125(16) Uiso 0.50 calc PR .
C3B C 0.4284(12) 0.0585(7) 0.3509(10) 0.098(3) Uiso 0.50 d P .
H3B1 H 0.4410(33) 0.0487(36) 0.4295(19) 0.125(16) Uiso 0.50 calc PR .
H3B2 H 0.4952(13) 0.0902(18) 0.3472(56) 0.125(16) Uiso 0.50 calc PR .
H3B3 H 0.4310(28) 0.0139(21) 0.3123(40) 0.125(16) Uiso 0.50 calc PR .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 P1 85.18(6) . . y
O1 Mo1 P1 94.82(6) . 3 y
O1 Mo1 P2 85.39(7) . . y
O1 Mo1 P2 94.61(7) . 3 y
P2 Mo1 P1 80.11(2) . . y
P2 Mo1 P1 99.89(2) . 3 y
C1 P1 C1A 101.66(14) . . y
C1 P1 C1G 102.64(14) . . y
C1A P1 C1G 103.56(13) . . y
Mo1 P1 C1 107.37(10) . . n
Mo1 P1 C1A 116.00(9) . . n
Mo1 P1 C1G 122.90(10) . . n
P1 C1 C2 121.8(2) . . y
P1 C1A C1B 120.8(2) . . n
P1 C1A C1F 120.0(2) . . n
P1 C1G C1M 122.0(3) . . n
P1 C1G C1H 119.0(2) . . n
C1F C1A C1B 119.0(3) . . n
C1A C1B C1C 120.2(3) . . n
C1B C1C C1D 120.3(3) . . n
C1C C1D C1E 120.2(3) . . n
C1D C1E C1F 120.2(3) . . n
C1E C1F C1A 120.1(3) . . n
C1M C1G C1H 118.9(3) . . n
C1G C1H C1I 119.8(4) . . n
C1H C1I C1K 121.0(4) . . n
C1I C1K C1L 120.1(4) . . n
C1K C1L C1M 119.7(4) . . n
C1L C1M C1G 120.6(4) . . n
C2 P2 C2A 101.77(14) . . y
C2 P2 C2G 102.39(14) . . y
C2A P2 C2G 103.14(13) . . y
Mo1 P2 C2 107.68(11) . . n
Mo1 P2 C2A 116.86(9) . . n
Mo1 P2 C2G 122.30(10) . . n
P2 C2 C1 121.5(2) . . y
P2 C2A C2B 119.1(2) . . n
P2 C2A C2F 122.0(2) . . n
P2 C2G C2M 121.9(3) . . n
P2 C2G C2H 119.0(2) . . n
C2F C2A C2B 118.9(3) . . n
C2A C2B C2C 120.7(3) . . n
C2B C2C C2D 120.0(3) . . n
C2C C2D C2E 120.1(3) . . n
C2D C2E C2F 120.2(3) . . n
C2E C2F C2A 120.0(3) . . n
C2M C2G C2H 119.0(3) . . n
C2G C2H C2I 120.5(3) . . n
C2H C2I C2K 120.0(4) . . n
C2I C2K C2L 120.1(4) . . n
C2K C2L C2M 120.4(4) . . n
C2L C2M C2G 120.0(4) . . n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.804(2) . y
Mo1 P1 2.5095(7) . y
Mo1 P2 2.5040(8) . y
P1 C1 1.826(3) . y
P1 C1A 1.820(3) . y
P1 C1G 1.820(3) . y
P2 C2 1.825(3) . y
P2 C2A 1.823(3) . y
P2 C2G 1.827(3) . y
C1 C2 1.309(4) . y
C1A C1B 1.388(4) . n
C1A C1F 1.377(4) . n
C1B C1C 1.378(4) . n
C1C C1D 1.365(5) . n
C1D C1E 1.363(5) . n
C1E C1F 1.390(5) . n
C1G C1H 1.361(5) . n
C1G C1M 1.383(5) . n
C1H C1I 1.388(5) . n
C1I C1K 1.348(6) . n
C1K C1L 1.359(6) . n
C1L C1M 1.382(5) . n
C2A C2B 1.381(4) . n
C2A C2F 1.384(4) . n
C2B C2C 1.382(5) . n
C2C C2D 1.370(5) . n
C2D C2E 1.369(5) . n
C2E C2F 1.390(5) . n
C2G C2H 1.373(4) . n
C2G C2M 1.386(5) . n
C2H C2I 1.383(5) . n
C2I C2K 1.364(6) . n
C2K C2L 1.364(6) . n
C2L C2M 1.379(5) . n
O3 C3A 1.188(12) . n
O3 C3B 1.230(12) . n
